CN103073028A - Magnetic nano-Turnbull's blue and its preparation method and use - Google Patents
Magnetic nano-Turnbull's blue and its preparation method and use Download PDFInfo
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- CN103073028A CN103073028A CN2012105613154A CN201210561315A CN103073028A CN 103073028 A CN103073028 A CN 103073028A CN 2012105613154 A CN2012105613154 A CN 2012105613154A CN 201210561315 A CN201210561315 A CN 201210561315A CN 103073028 A CN103073028 A CN 103073028A
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Abstract
The invention belongs to the technical field of Turnbull's blue synthesis and nano-materials and relates to a magnetic nano-Turnbull's blue and its preparation method and use. The preparation method of the magnetic nano-Turnbull's blue comprises that an iron imidazole magnetic ion-containing liquid and a potassium ferricyanide aqueous solution undergo a reaction in a solvent with magnetic stirring; and reaction products are separated and purified so that the magnetic nano-Turnbull's blue is obtained. The preparation method has simple processes and strong controllability, is suitable for large-scale production and has good application prospects.
Description
Technical field
The invention belongs to Teng Shi blue synthetic and technical field of nano material, particularly a kind of magnetic Nano Teng Shi indigo plant and its preparation method and application.
Background technology
Development along with world economy; the problem such as environment protection, food safety has become an important ring that concerns national economy; and rationally, effectively Monitoring techniques can reflect environmental quality and food Security Status and variation tendency in time, accurately, all sidedly, is key and the restrictive factor of prevention and control and improvement.
Traditional method such as GC, GC-FTIR, GC-MS, HPLC, LC-MS-MS, ICP-MS, the GC-atomic fluorescence, atomic absorption, (the Lee C such as microwave plasma, Yoon J, Von GU, et al. Oxidative degradation of nitrosodimethyl amine by conventional ozonation and the advanced oxidation process ozone/hydrogenperoxide. Water Research, 2007,41 (3): 581-590), all adopt offline mode, analysis speed is slow, complicated operation, required instrument is expensive, is unsuitable for on-the-spot fast monitored and continuous on-line analysis.Therefore, present various, complicated, micro-characteristics for current pollutent, set up and development continuously, online, field monitoring system fast, develop highly sensitive, high specificity, simple and efficient detection technique and means seem particularly important.
Electrochemical techniques are because advantage and characteristics such as high, the real-time online of environment compatibility is strong, controllability, multifunctionality and economy, playing an important role (Vecitis CD aspect current environment, food, biological monitoring and the improvement, Gao G, and Liu H. Electrochemical carbon nanotube filter for adsorption, desorption, and oxidation of aqueous dyes and anions. J. Phys. Chem. C, 2011,115 (9), 3621 – 3629).But it is not high that the electrochemical method weak point is used Electrode selectivity, and side reaction easily occurs, and reduces current efficiency; Electrode easily forms adsorption layer and oxide film and stained, and the life-span reduces; Monitoring sensitivity is limited; Be difficult to and original position analysis real-time, online to pollutent etc.
The development of sensor and acquisition of signal technology, remedied the deficiency of traditional electrical chemical monitoring, and along with the progress of Materials science receives publicity day by day, and become new lover (Danielle WK, Gabriel L, the et al. Electrochemical sensors and biosensors of FUTURE ENVIRONMENT, food, biological detection, Anal. Chem., 2012,84 (2), 685 – 707).Have been reported both at home and abroad at present and use the sensing technology exploration to carry out arsenide and sulfide, pesticide residue, waste water quality, biochemical oxygen demand (BOD) and ammonia nitrogen, phenolic comp ' ds pollution, the monitoring of the target compounds such as compound odorous (Ferdinando F, Luigia M, Giovanni PCM, et al. Thermostable esterase from alicyclobacillus acidocaldarius as biosensor for the detection of organophosphate pesticides. Anal. Chem., 2011,83 (5): 1530 – 1536), but all be in the very weak starting stage, especially face response stability poor, work-ing life is short, the problem such as expensive.Studies show that, the transverter that research and development have recognition function is core and the key of novel analytical instrument and analytical procedure.In other words, one of core key factor of restriction sensor widespread use is that design, exploitation are efficient, the novel sensing material of highly selective, such as conductive polymers, sol-gel, nano material, Surfactant Films and BLM etc., and this material has become the key for the treatment of in breaking through.
Magnetic ionic liquids not only has preferably the principal advantages such as thermostability, easily separated, good solubility, and externally-applied magnetic field is had magnetic response.These characteristics make the application of magnetic ionic liquids possess larger advantage and potentiality.From 2004 by the people such as Hayashi (S. Hayashi, H. Hamaguchi, Chem. Lett., 2004,1590,1591) since report [bmim] FeCl4 and the relevant nature thereof, obtained the extensive concern of researcher about the synthetic and application of this class magnetic ionic liquids.
Summary of the invention
The object of the present invention is to provide a kind of novel magnetic Nano Teng Shi indigo plant and its preparation method and application.
The technical solution used in the present invention is as follows:
A kind of magnetic Nano Teng Shi is blue, is made by laxative remedy: iron content imidazoles magnetic ionic liquids and saturated Hexacyanoferrate aqueous solutions of potassium react in solvent, under the magnetic agitation, and afterwards separation and purification obtains nano-magnetic Teng Shi indigo plant.
Described iron content imidazoles magnetic ionic liquids is preferably 1-butyl-3-Methylimidazole titanium tetrachloride salt or 1-octyl group-3-Methylimidazole titanium tetrachloride salt.
Described solvent is preferably ethanol, acetone or redistilled water.
Reaction times is advisable with 2-4h.
Described separation and purification is left standstill 24-48h after for reaction, isolates clear liquid, lower floor's mixture is carried out centrifugal, and the supernatant liquid after centrifugal is after supersound washing, and Air drying 12-24h obtains nano-magnetic Teng Shi behind 100-150 ℃ of vacuum-drying 4-6h blue afterwards.
Supersound washing adopts acetone, ethanol, intermediate water to carry out.Answer repetitive scrubbing colourless to supernatant liquor during washing.
Be preferable over 120-150 ℃ of vacuum-drying 3-5h.
Magnetic Nano Teng Shi indigo plant of the present invention has the solubility property that is insoluble to acetone, is insoluble in water and ethanol; Run into NaOH and become the tawny precipitation; Do not react with 30% hydrogen peroxide; In the hydrogen peroxide 30% under the impressed voltage condition, be converted into the tawny material, and follow Bubble formation.Be distributed in the water, magnet is had magnetic response.The easily separated purification of preparation method, stable, need not add the reunion that stablizer and dispersion agent can be avoided nanometer Teng Shi indigo plant in the reaction process; Preparation cycle is short, condition of normal pressure, equipment are simple.
Described magnetic Nano Teng Shi indigo plant has good application as sensing material, has excellent electrochemical activity.As can be used as the sensing material that nitrite is monitored, at environment, food and biomedical sector good application prospect is arranged.
Utilize the blue concentration of measuring nitrite anions of magnetic Nano Teng Shi, concrete grammar is as follows: the glass-carbon electrode of diameter 2-4mm is after polishing, ultrasonic cleaning, the 1.0-3.0mg/10mL nanometer Teng Shi indigo plant of 5-15 μ L/dehydrated alcohol dispersant liquid drop is applied on the glass-carbon electrode surface, dries under the infrared lamp and to get the blue modified electrode of Teng Shi; Adopt traditional three-electrode system, not have electroactive inorganic salt as supporting electrolyte, apply+1.6～-voltage of 1.6V, the oxidation current of record nitrite anions under the 50-150mV/s sweep velocity, and quantitative its concentration accordingly.
The present invention has following advantage with respect to prior art:
The blue preparation method of novel magnetic nanometer Teng Shi of the present invention is easy, controllability is strong, is produced on a large scale; Good application prospect is arranged.
Description of drawings
Fig. 1 is the AFM figure of magnetic Nano Teng Shi indigo plant of the present invention;
(A) the blue AFM figure that is coated onto after clean glass pane surface is dried that evenly drips of Teng Shi, the speck among the figure shows that the size distribution of Teng Shi indigo plant is between 80～120nm;
(B) the blue AFM three-dimensional plot of Teng Shi shows that this material is the combination of regular spike shape;
Fig. 2 is the infrared absorpting light spectra of the Tripotassium iron hexacyanide (a), Teng Shi blue (b), 1-butyl-3-Methylimidazole titanium tetrachloride salt (c);
Fig. 3 is element N1s and Fe2p in the Teng Shi basket of the present invention
1/2High resolution X-ray electronic spectrum (XPS) figure;
Fig. 4 is the cyclic voltammogram (CV) of the embodiment of the invention blue modified electrode of 1 described Teng Shi in 0.1MKCl;
Fig. 5 is that Teng Shi indigo plant of the present invention is to the response diagram of externally-applied magnetic field;
(A) aqueous dispersion liquid of Teng Shi indigo plant was placed magnet 0 hour;
(B) aqueous dispersion liquid of Teng Shi indigo plant was placed magnet 4 hours;
(C) aqueous dispersion liquid of Teng Shi indigo plant was placed magnet 4 hours, removed magnet;
Fig. 6 is the blue cyclic voltammogram (CV) of Teng Shi of the present invention;
(a) cyclic voltammogram of the blue modified electrode of Teng Shi in 0.1MKCl;
(b) the blue modified electrode of Teng Shi is at 30% H
2O
2After cyclic voltammetry scanning 20 is enclosed in the solution, the cyclic voltammogram of this modified electrode in 0.1MKCl;
Fig. 7 is the cyclic voltammogram (CV) that the blue modified electrode of Teng Shi of the present invention detects Sodium Nitrite:
(a) blank glass-carbon electrode is to 0.1MKCl+10
-3Mol/L NaNO
2Cyclic voltammogram;
(b) cyclic voltammogram of the blue modified electrode of Teng Shi in 0.1MKCl;
(c) the blue modified electrode of Teng Shi is in 0.1MKCl+10
-3Mol/L NaNO
2In cyclic voltammogram;
Fig. 8 is peak current and the NO that the blue modified electrode of Teng Shi of the present invention detects Sodium Nitrite
2 -The graph of a relation of concentration.
Embodiment
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited to this:
Get the 10mL redistilled water, add the Hexacyanoferrate potassium of capacity, ultra-sonic dispersion 2 minutes obtains saturated Hexacyanoferrate potassium solution.
Get 30mL acetone in the round-bottomed flask of 250mL, add 4mL [bmim] FeCl
4Dropwise add Hexacyanoferrate potassium saturated solution under the magnetic agitation and become blackish green to solution, continue to stir 2h, leave standstill 28h, isolate clear liquid, change in the centrifuge tube lower floor's mixture under the 8000r/min condition centrifugal 10min, inclining supernatant liquid, with acetone, intermediate water difference supersound washing synthetic, until supernatant liquor is colourless.Air drying (25 ℃) 12h changes 130 ℃ of vacuum-drying 4h in the test tube over to, takes out to place the moisture eliminator sealing to preserve.
Glass-carbon electrode Al with diameter 2mm
2O
3After the polishing, use respectively acetone, ethanol, redistilled water ultrasonic cleaning, obtain the good electrode of pre-treatment.1.0mg nanometer Teng Shi indigo plant is scattered in the 10mL dehydrated alcohol, this dispersion liquid 8 μ L drip and are applied on the above-mentioned electrode surface, and oven dry namely gets the blue modified electrode of Teng Shi under the infrared lamp.Adopt traditional three-electrode system, take the blue modified electrode of Teng Shi as working electrode, platinum electrode is to electrode, Ag/AgCl electrode take saturated KCl as reference liquid is reference electrode, it is supporting electrolyte that KCl does not have electroactive inorganic salt, add successively 0.1mmol/L, 0.3 mmol/L, 0.5 mmol/L, 0.7 the Sodium Nitrite of mmol/L, adopt the CHI650 electrochemical workstation, potentiostat applies+1.6～-voltage of 1.6V, the oxidation current of record nitrite anions under the 50mV/s sweep velocity, take electric current as ordinate zou, concentration is that the X-coordinate mapping obtains typical curve, the sample of unknown concentration is tested its oxidation current under the same conditions, can analyze corresponding concentration on typical curve.The method can be used for the mensuration of the sample nitrites such as environment, food.
Get the 15mL redistilled water, add the Hexacyanoferrate potassium of capacity, ultra-sonic dispersion 4 minutes obtains saturated Hexacyanoferrate potassium solution.
Get 20mL acetone in the round-bottomed flask of 250mL, add 3mL [bmim] FeCl
4Dropwise add Hexacyanoferrate potassium saturated solution under the magnetic agitation and become blackish green to solution, continue to stir 2h, leave standstill 24h, isolate clear liquid, lower floor's mixture is changed in the centrifuge tube in the centrifugal 15min of 6000r/min, inclining supernatant liquid, with acetone, intermediate water difference supersound washing synthetic, until supernatant liquor is colourless.Air drying (20 ℃) 24h changes 120 ℃ of vacuum-drying 5h in the test tube over to, takes out to place the moisture eliminator sealing to preserve.
Glass-carbon electrode Al with diameter 3mm
2O
3After the polishing, use respectively acetone, ethanol, redistilled water ultrasonic cleaning, obtain the good electrode of pre-treatment.2.0mg nanometer Teng Shi indigo plant is scattered in the 10mL dehydrated alcohol, this dispersion liquid 10 μ L drip and are applied on the above-mentioned electrode surface, and oven dry namely gets the blue modified electrode of Teng Shi under the infrared lamp.Adopt traditional three-electrode system, take the blue modified electrode of Teng Shi as working electrode, platinum electrode is to electrode, Ag/AgCl electrode take saturated KCl as reference liquid is reference electrode, KNO3 is supporting electrolyte, the Sodium Nitrite that adds successively 0.1mmol/L, 0.3 mmol/L, 0.5 mmol/L, 0.7 mmol/L, adopt CHI650 electrochemical workstation, potentiostat apply+1.6～-voltage of 1.6V, the oxidation current of record nitrite anions under the 100mV/s sweep velocity.Take electric current as ordinate zou, concentration obtains typical curve as X-coordinate mapping, the sample of unknown concentration is tested its oxidation current under the same conditions, can analyze corresponding concentration on typical curve.The method can be used for the mensuration of the sample nitrites such as environment, food.
Get the 20mL redistilled water, add the Hexacyanoferrate potassium of capacity, ultra-sonic dispersion 5 minutes obtains saturated Hexacyanoferrate potassium solution.
Get 40mL acetone in the round-bottomed flask of 500mL, add 5mL [bmim] FeCl
4Dropwise add Hexacyanoferrate potassium saturated solution under the magnetic agitation and become blackish green to solution, continue to stir 3h, leave standstill 36h, isolate clear liquid, lower floor's mixture is changed in the centrifuge tube in the centrifugal 8min of 10000r/min, inclining supernatant liquid, with acetone, intermediate water difference supersound washing synthetic, until supernatant liquor is colourless.Air drying (23 ℃) 14h changes 140 ℃ of vacuum-drying 3.5h in the test tube over to, takes out to place the moisture eliminator sealing to preserve.
Glass-carbon electrode Al with diameter 4mm
2O
3After the polishing, use respectively acetone, ethanol, redistilled water ultrasonic cleaning, obtain the good electrode of pre-treatment.3.0mg nanometer Teng Shi indigo plant is scattered in the 10mL dehydrated alcohol, this dispersion liquid 10 μ L drip and are applied on the above-mentioned electrode surface, and oven dry namely gets the blue modified electrode of Teng Shi under the infrared lamp.Adopt traditional three-electrode system, take the blue modified electrode of Teng Shi as working electrode, platinum electrode is to electrode, Ag/AgCl electrode take saturated KCl as reference liquid is reference electrode, KCl is supporting electrolyte, add successively 0.1mmol/L, 0.3 mmol/L, 0.5 mmol/L, 0.7 the Sodium Nitrite of mmol/L, adopt electrochemical workstation, potentiostat applies+1.6～-voltage of 1.6V, the oxidation current of record nitrite anions is take electric current as ordinate zou under the 150mV/s sweep velocity, concentration is that the X-coordinate mapping obtains typical curve, the sample of unknown concentration is tested its oxidation current under the same conditions, can analyze corresponding concentration on typical curve.The method can be used for the mensuration of the sample nitrites such as environment, food.
Get the 20mL redistilled water, add the Hexacyanoferrate potassium of capacity, ultra-sonic dispersion 4 minutes obtains saturated Hexacyanoferrate potassium solution.
Get 50mL acetone in the round-bottomed flask of 500mL, add 5mL [bmim] FeCl
4Dropwise add Hexacyanoferrate potassium saturated solution under the magnetic agitation and become blackish green to solution, continue to stir 4h, leave standstill 48h, isolate clear liquid, lower floor's mixture is changed in the centrifuge tube in the centrifugal 12min of 9000r/min, inclining supernatant liquid, with acetone, intermediate water difference supersound washing synthetic, until supernatant liquor is colourless.Air drying (20 ℃) 12h changes 150 ℃ of vacuum-drying 3h in the test tube over to, takes out to place the moisture eliminator sealing to preserve.
Glass-carbon electrode Al with diameter 3mm
2O
3After the polishing, use respectively acetone, ethanol, redistilled water ultrasonic cleaning, obtain the good electrode of pre-treatment.1.0mg nanometer Teng Shi indigo plant is scattered in the 10mL dehydrated alcohol, this dispersion liquid 15 μ L drip and are applied on the above-mentioned electrode surface, and oven dry namely gets the blue modified electrode of Teng Shi under the infrared lamp.Adopt traditional three-electrode system, take the blue modified electrode of Teng Shi as working electrode, platinum electrode is to electrode, Ag/AgCl electrode take saturated KNO3 as reference liquid is reference electrode, KCl is supporting electrolyte, add successively 0.1mmol/L, 0.3 mmol/L, 0.5 mmol/L, 0.7 the Sodium Nitrite of mmol/L, adopt electrochemical workstation, potentiostat applies+1.6～-voltage of 1.6V, the oxidation current of record nitrite anions is take electric current as ordinate zou under the 100mV/s sweep velocity, concentration is that the X-coordinate mapping obtains typical curve, the sample of unknown concentration is tested its oxidation current under the same conditions, can analyze corresponding concentration on typical curve.The method can be used for the mensuration of the sample nitrites such as environment, food.
Above-described embodiment is the preferred embodiment of the present invention, but embodiments of the present invention are not restricted to the described embodiments, and the change that other any the present invention of not deviating from does all should be the substitute mode of equivalence, is included within protection scope of the present invention.
Claims (9)
1. a magnetic Nano Teng Shi is blue, it is characterized in that, is made by laxative remedy: iron content imidazoles magnetic ionic liquids and saturated Hexacyanoferrate aqueous solutions of potassium react in solvent, under the magnetic agitation, and afterwards separation and purification obtains nano-magnetic Teng Shi indigo plant.
2. the preparation method of magnetic Nano Teng Shi indigo plant is characterized in that, iron content imidazoles magnetic ionic liquids and saturated Hexacyanoferrate aqueous solutions of potassium react in solvent, under the magnetic agitation, and it is blue that afterwards separation and purification obtains nano-magnetic Teng Shi.
3. the preparation method of magnetic Nano Teng Shi indigo plant as claimed in claim 2 is characterized in that, described iron content imidazoles magnetic ionic liquids is 1-butyl-3-Methylimidazole titanium tetrachloride salt or 1-octyl group-3-Methylimidazole titanium tetrachloride salt.
4. the preparation method of magnetic Nano Teng Shi indigo plant as claimed in claim 2 is characterized in that, described solvent is ethanol, acetone or redistilled water.
5. the preparation method of magnetic Nano Teng Shi indigo plant as claimed in claim 2 is characterized in that, the reaction times is 2-4h.
6. the preparation method of magnetic Nano Teng Shi indigo plant as claimed in claim 2, it is characterized in that, described separation and purification is left standstill 24-48h after reacting, isolate clear liquid, carry out lower floor's mixture centrifugal, supernatant liquid after centrifugal is after supersound washing, and Air drying 12-24h obtains nano-magnetic Teng Shi indigo plant behind 100-150 ℃ of vacuum-drying 4-6h afterwards.
7. the preparation method of magnetic Nano Teng Shi indigo plant as claimed in claim 6 is characterized in that, supersound washing adopts acetone, ethanol, intermediate water to carry out.
8. the described magnetic Nano Teng Shi of claim 1 indigo plant is as the application of sensing material.
9. magnetic Nano Teng Shi indigo plant as claimed in claim 8 is as the application of sensing material, it is characterized in that, utilize the blue concentration of measuring nitrite anions of magnetic Nano Teng Shi, method is as follows: the glass-carbon electrode of diameter 2-4mm is after polishing, ultrasonic cleaning, the 1.0-3.0mg/10mL nanometer Teng Shi indigo plant of 5-15 μ L/dehydrated alcohol dispersant liquid drop is applied on the glass-carbon electrode surface, dries under the infrared lamp and to get the blue modified electrode of Teng Shi; Adopt traditional three-electrode system, not have electroactive inorganic salt as supporting electrolyte, apply+1.6～-voltage of 1.6V, the oxidation current of record nitrite anions under the 50-150mV/s sweep velocity, and quantitative its concentration accordingly.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113624815A (en) * | 2021-06-30 | 2021-11-09 | 江西师范大学 | Double-signal miRNA-21 detection method based on three-dimensional DNA Walker and Turnbull's blue |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113624815A (en) * | 2021-06-30 | 2021-11-09 | 江西师范大学 | Double-signal miRNA-21 detection method based on three-dimensional DNA Walker and Turnbull's blue |
| CN113624815B (en) * | 2021-06-30 | 2023-04-11 | 江西师范大学 | Double-signal miRNA-21 detection method based on three-dimensional DNA Walker and Turnbull's blue |
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